CN106159245A - A kind of preparation method of graphene battery negative plate - Google Patents

A kind of preparation method of graphene battery negative plate Download PDF

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Publication number
CN106159245A
CN106159245A CN201610862742.4A CN201610862742A CN106159245A CN 106159245 A CN106159245 A CN 106159245A CN 201610862742 A CN201610862742 A CN 201610862742A CN 106159245 A CN106159245 A CN 106159245A
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graphene
negative plate
preparation
battery negative
solution
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钟静琴
钟静清
韦晗
陶佳
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Liuzhou Shentong Automobile Technology Co Ltd
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Liuzhou Shentong Automobile Technology Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention relates to the preparation method of a kind of graphene battery negative plate, it includes being placed in ice-water bath sulfuric acid solution and salpeter solution, adds graphite raw material and solid potassium permanganate；After temperature is increased to room temperature, adds distilled water reaction and obtain graphene oxide；Take graphene oxide to be placed in the container filling HCl solution, disperse with deionized water and stir；Then said mixture is placed in microexplosion reactor, adds KClO3Solution, H2O2Complete microexplosion reaction, obtain stannic oxide/graphene nano volume；By stannic oxide/graphene nano volume and SnCl4Soluble in water, it is subsequently adding reducing agent reaction and obtains SnO2/ graphene nano volume composite negative pole material, then makes negative plate.The present invention is dioxide composite tin material on graphene nano is rolled up, the material property prepared has more excellent hydrogen storage property compared to Graphene and tin dioxide composite material, as the negative pole of new energy car battery, it is greatly improved the serviceability of battery, extends the service life of battery.

Description

A kind of preparation method of graphene battery negative plate
Technical field
The present invention relates to automobile batteries negative material, the preparation method of a kind of graphene battery negative plate.
Background technology
The Graphene of curling causes the attention of some researcheres as a kind of novel nanostructured, and entitled Graphene is received Rice is rolled up, and its discovery can trace back to nineteen sixty, and graphene nano volume has quasi-one-dimentional structure, is by plane Graphene helix-coil Becoming, the size of its radius depends on the size of graphite and the curvature of curling.Additionally, the two ends of non-closed state and outer edge can To improve the hydrogen storage ability of graphene nano volume, it is used as the electrode material of ultracapacitor or battery, especially as The cell negative electrode material of new-energy automobile, the R&D direction of Cheng Xin；Between graphene nano volume layer under key effect, adjustable interlayer Away from electron transfer and the optical characteristics that can affect graphene nano volume.Therefore, graphene nano rolls up oneself becomes graphene-based nanometer One of study hotspot of material.
At present, preparation and the application of graphene nano volume far lag behind Graphene and CNT, and its research is the most only concentrated At structure and the Theoretical Calculation of performance and computer simulation.Chemical method is used to synthesize the intercalation chemical combination of graphite and metal K Thing, then to its supersound process, prepare first graphene nano volume, and propose graphene nano volume have than Graphene more Significantly hydrogen storage ability and have the hypothesis of super large capacitor of six times of Graphenes.The method must complicated at anhydrous and oxygen-free etc. and Carry out under harsh conditions, therefore, in extensive preparation with application aspect by a definite limitation.Additionally, it is multiple about SnO2/ Graphene The preparation report of condensation material is a lot, but concrete SnO2/ graphene nano volume composite really has no record.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides one and can prepare SnO2/ graphene nano volume Compound Negative The preparation method of pole piece, the method is simple, and prepared material has hydrogen storage property and the capacitive property of excellence.
The present invention solves the technical scheme that above-mentioned technical problem used: the preparation side of a kind of graphene battery negative plate Method, it comprises the following steps:
(1) sulfuric acid solution and salpeter solution are placed in ice-water bath stirring, are subsequently adding graphite raw material and solid potassium permanganate, and Continue stirring；
(2) after temperature is increased to room temperature, withdraw ice-water bath, and add distilled water reaction, then sucking filtration, obtain graphite oxide Alkene；
(3) take above-mentioned graphene oxide, be placed in filling in the container of HCl solution, disperse with deionized water and stir；
(4) then said mixture is placed in microexplosion reactor, adds KClO3Solution, adds H2O2Complete microexplosion reaction, Obtain the stannic oxide/graphene nano volume with crimped configuration；
(5) by above-mentioned stannic oxide/graphene nano volume and SnCl4By certain mass than mix homogeneously soluble in water；
(6) it is subsequently adding reducing agent reaction, and filters, wash, be dried, obtain SnO2/ graphene nano volume negative material；
(7) above-mentioned SnO2/ graphene nano volume composite negative pole material, binding agent, conductive agent and appropriate water mix and blend are ground Mill, it is thus achieved that cathode size；
(8) cathode size is coated on Copper Foil, and dries, roll-in, cut and obtain negative plate.
As preferably, the mass concentration of described sulfuric acid solution is 96%, and consumption is 80-100 mL；The mass concentration of nitric acid is 96%, consumption is 20-40 mL；The quality of graphite raw material is 2-3g, and the quality of solid potassium permanganate is 13-14g.
As preferably, described graphene oxide consumption is 0.5-1g, and the concentration of HCl solution is 1mol/L, and consumption is 60- 100mL。
As preferably, disperse with deionized water and use agitator to stir 4-13h.
As preferably, KClO3Solution uses the mode being added dropwise over, and concentration is 1mol/L, and consumption is 10-20mL.
As preferably, KClO3After solution is added dropwise to complete, add the H of 50-100mL30%2O2。
As preferably, stannic oxide/graphene nano is rolled up and SnCl4Mass ratio be (2-10).
As preferably, reducing agent uses hydrazine hydrate or sodium borohydride, response time 10-24h.
As preferably, SnO2/ graphene nano volume composite negative pole material, binding agent, the mass ratio of conductive agent are (7-9): 1:1。
As preferably, cathode size is coated on Copper Foil with the speed of 3-5m/min at a temperature of 100-180 DEG C, so After the Copper Foil of this coating toasted at a temperature of 100-180 DEG C 6-8h.
As can be known from the above technical solutions, the present invention is dioxide composite tin material on graphene nano is rolled up, and prepares Material property has more excellent hydrogen storage property compared to Graphene and tin dioxide composite material, as new-energy automobile electricity The negative pole in pond, is greatly improved the serviceability of battery, extends the service life of battery.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention, But it is not as a limitation of the invention.
A kind of preparation method of graphene battery negative plate, it comprises the following steps:
Sulfuric acid solution and the salpeter solution that 20-40 mL mass concentration is 96% that 80-100 mL mass concentration is 96% are placed in ice Stirred in water bath, is subsequently adding 2-3g graphite raw material and 13-14g solid potassium permanganate, and continues stirring；Treat that temperature is increased to room Wen Hou, withdraws ice-water bath, and adds distilled water reaction, then sucking filtration, obtain graphene oxide；Take 0.5-1g graphene oxide to put In filling in the container of HCl solution of 60-100mL 1mol/L, disperse with deionized water and use agitator to stir 4-13h； Then said mixture is placed in microexplosion reactor, is added dropwise over the KClO of 10-20mL 1mol/L3Solution, KClO3Solution The H2O2 adding 50-100mL30% after being added dropwise to complete completes microexplosion reaction, and the graphene oxide obtaining having crimped configuration is received Rice volume；Then by above-mentioned stannic oxide/graphene nano volume and SnCl4(2-10) mix homogeneously soluble in water, is subsequently adding in mass ratio Reducing agent hydrazine hydrate or sodium borohydride, after reaction 10-24h, filter and use deionized water cyclic washing, being dried the most available SnO2/ graphene nano volume composite negative pole material；Above-mentioned SnO2/ graphene nano is rolled up composite negative pole material, binding agent, conduction Agent by the mass ratio of (7-9): 1:1 and is ground with appropriate water mix and blend, it is thus achieved that cathode size；By cathode size at 100- It is coated on Copper Foil with the speed of 3-5m/min at a temperature of 180 DEG C, then by the Copper Foil of this coating the temperature of 100-180 DEG C Lower baking 6--8h；Thus ensure Painting effect.Copper Foil after drying carries out roll-in respectively, then cuts into given size Negative plate；The compacted density of the negative plate after roll-in is 1.2-1.4g/cm3.It is said that in general, compacted density is the biggest, the appearance of battery Amount can be the highest, but cross conference and cause contact between particle closely, to make distance diminish, and when injecting enough electrolyte, absorbs The space of electrolyte diminishes, and affects the dynamic performance of material.
Embodiment 1
Sulfuric acid solution that 80mL mass concentration is 96% and salpeter solution that 20 mL mass concentrations are 96% are placed in ice-water bath and stir Mix, be subsequently adding 2g graphite raw material and 13g solid potassium permanganate, and continue stirring；After temperature is increased to room temperature, withdraw frozen water Bath, and add distilled water reaction, then sucking filtration, obtain graphene oxide；Take graphene oxide and the 60 mL 1mol/ of 0.5g In LHCl flask, with deionized water dispersion and stir 4h with agitator, then the mixture obtained be placed in microexplosion reactor, It is added dropwise over 10mL 1mol/L KClO3In microexplosion reactor, after being added dropwise to complete, add the H of 50mL30%2O2Complete microexplosion Reaction, finally gives the stannic oxide/graphene nano volume with crimped configuration；By prepared stannic oxide/graphene nano volume and SnCl4Press Mass ratio 1:5 mix homogeneously soluble in water, the rear reducing agent hydrazine hydrate that adds, after reaction 10h, filters and repeatedly washes with deionized water Wash, be dried to obtain SnO2/ graphene nano volume composite；By above-mentioned SnO2/ graphene nano is rolled up composite negative pole material, is glued Knot agent, conductive agent are pressed the mass ratio of 7:1:1 and grind with appropriate water mix and blend, it is thus achieved that cathode size；Cathode size is existed It is coated on Copper Foil with the speed of 3m/min at a temperature of 100 DEG C, then the Copper Foil of this coating is toasted at a temperature of 100 DEG C 6h, then roll-in, cut and obtain negative plate.Test this negative plate to obtain: electrode is at 600mA g-1Charging and discharging currents density, Cycle performance under 0.05-3.0 V voltage shows bigger performance improvement, and discharge capacity reaches 2770 mAh g first-1, fill Capacitance is 1540 mAh g-1, initial coulomb efficiency about 56%, discharge capacity about 820mAh g after 100 circulations-1。
Embodiment 2
Sulfuric acid solution and the salpeter solution that 30 mL mass concentrations are 96% that 90 mL mass concentrations are 96% are placed in ice-water bath Stirring, is subsequently adding 2.5g graphite raw material and 13.5g solid potassium permanganate, and continues stirring；After temperature is increased to room temperature, remove Walk ice-water bath, and add distilled water reaction, then sucking filtration, obtain graphene oxide；Take graphene oxide and 80 mL of 1g In 1mol/LHCl flask, with deionized water dispersion and stir 8h with agitator, then the mixture obtained is placed in microexplosion reaction In device, it is added dropwise over 20mL 1mol/L KClO3In microexplosion reactor, after being added dropwise to complete, add the H of 70mL30%2O2Complete Microexplosion is reacted, and finally gives the stannic oxide/graphene nano volume with crimped configuration；By prepared stannic oxide/graphene nano volume and SnCl4By 1:2 than mix homogeneously soluble in water, the rear borane reducing agent sodium hydride that adds, after reaction 15h, filters and uses deionized water Cyclic washing, is dried to obtain SnO2/ graphene nano volume composite；By above-mentioned SnO2/ graphene nano volume composite negative pole material Material, binding agent, conductive agent are pressed the mass ratio of 8:1:1 and grind with appropriate water mix and blend, it is thus achieved that cathode size；Negative pole is starched Material is coated on Copper Foil with the speed of 4m/min, at a temperature of 150 DEG C then by the Copper Foil of this coating at a temperature of 140 DEG C Baking 7h, then roll-in, cut and obtain negative plate.Test this negative plate to obtain: electrode is at 600mA g-1Charging and discharging currents close Cycle performance under degree, 0.05-3.0 V voltage shows bigger performance improvement, and discharge capacity reaches 2580 mAh g first-1, Charging capacity is 1720 mAh g-1, initial coulomb efficiency about 67%, after 100 circulations, discharge capacity is from 170mAh g-1Improve to 920mAh g-1。
Embodiment 3
Sulfuric acid solution and the salpeter solution that 40 mL mass concentrations are 96% that 100 mL mass concentrations are 96% are placed in ice-water bath Stirring, is subsequently adding 3g graphite raw material and 14g solid potassium permanganate, and continues stirring；After temperature is increased to room temperature, withdraw ice Water-bath, and add distilled water reaction, then sucking filtration, obtain graphene oxide；Take graphene oxide and the 100 mL 1mol/ of 1g In LHCl flask, with deionized water dispersion and stir 13h with agitator, then the mixture obtained is placed in microexplosion reactor In, it is added dropwise over 10mL 1mol/L KClO3In microexplosion reactor, after being added dropwise to complete, add the H of 50-100mL30%2O2Complete Become microexplosion reaction, finally give the stannic oxide/graphene nano volume with crimped configuration；By prepared stannic oxide/graphene nano volume and SnCl4The mix homogeneously soluble in water of 1:10 in mass ratio, the rear reducing agent hydrazine hydrate that adds, after reaction 24h, filters and uses deionization Water cyclic washing, is dried to obtain SnO2/ graphene nano volume composite；By above-mentioned SnO2/ graphene nano volume composite negative pole Material, binding agent, conductive agent are pressed the mass ratio of 9:1:1 and grind with appropriate water mix and blend, it is thus achieved that cathode size；By negative pole Slurry is coated on Copper Foil with the speed of 5m/min at a temperature of 180 DEG C, then by the Copper Foil of this coating the temperature of 180 DEG C Lower baking 8h, then roll-in, cut and obtain negative plate.Test this negative plate to obtain: electrode is at 600mA g-1Charging and discharging currents close Cycle performance under degree, 0.05-3.0 V voltage shows bigger performance improvement, and discharge capacity reaches 2470 mAh g first-1, Charging capacity is 1460 mAh g-1, initial coulomb efficiency about 60%, after 100 circulations, discharge capacity is 890mAh g-1。
The technical scheme provided the embodiment of the present invention above is described in detail, specific case used herein Principle and embodiment to the embodiment of the present invention are set forth, and the explanation of above example is only applicable to help to understand this The principle of inventive embodiments；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, in specific embodiment party All will change in formula and range of application, in sum, this specification content should not be construed as limitation of the present invention.

Claims (10)

1. a preparation method for graphene battery negative plate, it comprises the following steps:
(1) sulfuric acid solution and salpeter solution are placed in ice-water bath stirring, are subsequently adding graphite raw material and solid potassium permanganate, and Continue stirring；
(2) after temperature is increased to room temperature, withdraw ice-water bath, and add distilled water reaction, then sucking filtration, obtain graphite oxide Alkene；
(3) take above-mentioned graphene oxide, be placed in filling in the container of HCl solution, disperse with deionized water and stir；
(4) then said mixture is placed in microexplosion reactor, adds KClO3Solution, adds H2O2Complete microexplosion reaction, Obtain the stannic oxide/graphene nano volume with crimped configuration；
(5) by above-mentioned stannic oxide/graphene nano volume and SnCl4By certain mass than mix homogeneously soluble in water；
(6) it is subsequently adding reducing agent reaction, and filters, wash, be dried, obtain SnO2/ graphene nano volume negative material；
(7) above-mentioned SnO2/ graphene nano volume composite negative pole material, binding agent, conductive agent and appropriate water mix and blend are ground Mill, it is thus achieved that cathode size；
(8) cathode size is coated on Copper Foil, and dries, roll-in, cut and obtain negative plate.
The preparation method of graphene battery negative plate the most according to claim 1, it is characterised in that: the matter of described sulfuric acid solution Amount concentration is 96%, and consumption is 80-100 mL；The mass concentration of nitric acid is 96%, and consumption is 20-40 mL；The quality of graphite raw material For 2-3g, the quality of solid potassium permanganate is 13-14g.
The preparation method of graphene battery negative plate the most according to claim 1, it is characterised in that: described graphene oxide is used Amount is 0.5-1g, and the concentration of HCl solution is 1mol/L, and consumption is 60-100mL.
The preparation method of graphene battery negative plate the most according to claim 3, it is characterised in that: disperse also with deionized water Use agitator stirring 4-13h.
The preparation method of graphene battery negative plate the most according to claim 4, it is characterised in that: KClO3Solution uses dropwise The mode added, concentration is 1mol/L, and consumption is 10-20mL.
The preparation method of graphene battery negative plate the most according to claim 5, it is characterised in that: KClO3Solution is added dropwise to complete After, add the H of 50-100mL30%2O2。
The preparation method of graphene battery negative plate the most according to claim 6, it is characterised in that: stannic oxide/graphene nano is rolled up With SnCl4Mass ratio be 1:(2-10).
The preparation method of graphene battery negative plate the most according to claim 1, it is characterised in that: reducing agent uses hydrazine hydrate Or sodium borohydride, response time 10-24h.
The preparation method of graphene battery negative plate the most according to claim 1, it is characterised in that: SnO2/ graphene nano Volume composite negative pole material, binding agent, the mass ratio of conductive agent are (7-9): 1:1.
The preparation method of graphene battery negative plate the most according to claim 1, it is characterised in that: cathode size is existed It is coated on Copper Foil with the speed of 3-5m/min at a temperature of 100-180 DEG C, then by the Copper Foil of this coating at 100-180 DEG C At a temperature of toast 6-8h.
CN201610862742.4A 2016-09-29 2016-09-29 A kind of preparation method of graphene battery negative plate Pending CN106159245A (en)

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